CN109706479A - A kind of sheet V3S4Preparation and its electrocatalysis characteristic application - Google Patents
A kind of sheet V3S4Preparation and its electrocatalysis characteristic application Download PDFInfo
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- CN109706479A CN109706479A CN201811591304.4A CN201811591304A CN109706479A CN 109706479 A CN109706479 A CN 109706479A CN 201811591304 A CN201811591304 A CN 201811591304A CN 109706479 A CN109706479 A CN 109706479A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a kind of sheet V3S4The preparation method of elctro-catalyst and its application in terms of cracking aquatic products hydrogen catalyst as electro-catalysis.Vanadium disulfide is more and more paid close attention to by people in recent years as a kind of stratified material.However about V3S4Report it is few.The present invention obtains sheet by hydro-thermal-calcining two-step method, materials chemistry form it is uniform and in full PH electrolyte the high V of electro catalytic activity, stability3S4Produce hydrogen elctro-catalyst.
Description
Technical field
The present invention relates to nano-powder preparation technical fields, and in particular to a kind of sheet V3S4The preparation method of elctro-catalyst.
Background technique
Since the seventies, hydro carbons energy carrier molecular hydrogen is had been a hot spot of research, many merits having due to it:
With hydrocarbon fuels by-product CO2It compares, with big energy per mass density, cleans by-product water, content is rich
It is rich.On the other hand, hydrogen is typically found in compound, and therefrom we can separate hydrogen.The separating technology being widely used is steam
Conversion method, but it depends on fossil fuel, can generate CO2.In cleaning, renewable and without CO2In the water treatment technology of generation,
It is one of most promising technique that water-splitting, which produces hydrogen,.Most efficiently producing hydrogen catalyst is platinum, but its global resources is limited, difficult
To meet energy demand.Therefore, alternative catalysts are proposed with strong requirement: the element of rich content, high electrochemistry is living
Stability under property-i.e. low overpotential and operating condition.Transient metal sulfide elctro-catalyst, layer structure MoS2It is most
Representative transient metal chalcogenide compound, WS2As MoS2Heterogeneous isomorphism body, they have similar physics and change
Learn property.It is found that the transient metal chalcogenide compound of some non-laminar structures also has preferable HER catalytic activity, such as
The sulfide of Fe, Co, Ni and V, vanadic sulfide receive more and more people's as a kind of important layered inorganic material in recent years
Concern, and its application has been directed to responding ability, catalysis characteristics, hydrogen storage property, lubrication property and the lithium-ion electric of moisture
The fields such as the electrochemical properties of pond electrode material [Zhang Y, WuX.Vanadium sulfide nanoribbons:
Electronic and magnetic properties[J]. Physics Letters A,2013,377(43):3154-
3157]。
Application No. is a kind of Chinese patent of CN105932279A " nano bar-shape V3S4Preparation method and application " by vanadium source
Solution carries out hydro-thermal reaction, obtains barium oxide nano material, is then blended in tube furnace vanadium with sulphur and calcines, will forge
Washes clean, collection, drying after sample cooling after burning.The nano bar-shape V prepared3S4Be mainly used for ferromagnetic material and lithium/
The application of sodium ion battery electrode material.
This work has prepared a kind of sheet V by heat treating process after first hydro-thermal3S4Elctro-catalyst is mainly used in electricity and urges
Change field.
Summary of the invention
The invention discloses be prepared for a kind of sheet V with hydro-thermal-calcining two-step method3S4The preparation method of elctro-catalyst and its
Application in terms of cracking aquatic products hydrogen catalyst as electro-catalysis.
In order to achieve the above object, the present invention adopts the following technical scheme:
Step 1: vanadium source is dissolved in oxalic acid solution first, and pH value of solution is adjusted to alkalinity, hydro-thermal reaction is carried out, obtains a kind of vanadium
Oxide-based nanomaterial；By product washes clean, collects and be dried in vacuo.
Step 2: the air-tightness of tube furnace is checked；Barium oxide and sulphur source that molar ratio is 1:9 ~ 1:12 are put into tubular type
It is calcined in atmosphere furnace, temperature range is 700-900 DEG C, soaking time 2-3h, and heating rate is 5-10 DEG C/min, is obtained
Powder is carried out cooling, washs dry, collection, grinding by black powder.
Compared with the prior art, the present invention at least has following beneficial effect:
1) pH value for adjusting solution, is prepared for the V of sheet with hydro-thermal-calcining two-step method later3S4Nano-powder controls hydro-thermal
The temperature and time of reaction, may be implemented to VO2The control of appearance structure；
2) this method has many advantages, such as that simple process, raw material are cheap, at low cost, yield is high, is suitble to large-scale production；
3) V of this method preparation3S4Nano material chemical composition is uniform, and purity and crystallinity are all higher；
4) vanadic sulfide of this method preparation is a kind of novel water-splitting production hydrogen elctro-catalyst, in full pH value range (0~14), all
Show certain production hydrogen catalysis activity.
Detailed description of the invention:
Fig. 1 is VO prepared by the embodiment of the present invention 12X-ray diffraction (XRD) map；
Fig. 2 is V prepared by the embodiment of the present invention 13S4X-ray diffraction (XRD) map；
Fig. 3 is VO prepared by the embodiment of the present invention 22Scanning electron microscope (SEM) picture of nano-powder；
Fig. 4 is sheet V prepared by the embodiment of the present invention 33S4Scanning electron microscope (SEM) picture；
Fig. 5 is sheet V prepared by the embodiment of the present invention 43S4Production hydrogen LSV test chart under PH=0；
Fig. 6 is sheet V prepared by the embodiment of the present invention 43S4Production hydrogen LSV test chart under PH=7；
Fig. 7 is sheet V prepared by the embodiment of the present invention 43S4Production hydrogen LSV test chart under PH=14.
Specific embodiment
With reference to the accompanying drawing and embodiment invention is further described in detail, it should be appreciated that below these examples only
Illustrate and not limit the scope of the present invention.Here it will be understood that the ability after having read the content of the invention authorized
Field technique personnel can make any change or modification to the present invention, these equivalences equally fall within the application the appended claims institute
The range of restriction.
Embodiment 1
Step 1: the oxalic acid for weighing 4mmol dissolves in the deionized water of 40mL, and two drop ammonium hydroxide are added dropwise, after magnetic agitation 30min
To solution A；Weigh the V of 2mmol2O5It is dissolved in solution A, magnetic agitation 30min obtains solution B.
Step 2: configured solution B is poured into reaction polytetrafluoroethyllining lining, and the packing ratio of reaction kettle is 80%, and
Liner is fitted into outer kettle, is placed it in baking oven after fixing, reaction condition is to keep the temperature for 24 hours at 180 DEG C.
Step 3: water heating kettle cooled to room temperature after to hydro-thermal reaction pours out reaction solution deionized water, anhydrous
Ethyl alcohol is respectively washed 3 times.It is dried for 24 hours by sample collection after suction filtration and under the conditions of 60 DEG C of vacuum, VO can be obtained2Nano material.
Step 4: the molar ratio of control barium oxide and thioacetamide is 1:9, and two kinds of raw materials are laid in porcelain boat respectively
Porcelain boat is placed in tube-type atmosphere furnace by both ends, and in two furnace plugs of pipe both ends each side.
Step 5: being passed through inert gas into pipe, then carries out 8 pumping tonifying Qi, drains inner air tube, and last time is taken out
No longer tonifying Qi after gas, control intraductal atmospheric pressure are -1 ~ 0MPa；When air pressure is -1 ~ 0MPa, with the heating speed of 5 ~ 10 DEG C/min
Rate rises to 700 DEG C, and keeps the temperature 3h；After heat preservation, air valve is opened immediately, inert gas is passed through with 700 ~ 800sccm air-flow, is arranged
The sulfur vapor generated in insulating process out will guarantee that cooling carries out under argon gas stream later.
Step 6: calcined samples with water and dehydrated alcohol are respectively washed 3 times, and drying for 24 hours, can be obtained at 60 DEG C
V3S4Nano material.
Fig. 1 is VO prepared by the embodiment of the present invention 12X-ray diffraction (XRD) map；It can be seen that the diffraction of sample is special
Levying peak can index VO2。
Fig. 2 is V prepared by the embodiment of the present invention 13S4X-ray diffraction (XRD) map, it can be seen that the diffraction of sample is special
Levying peak can index V3S4, diffraction maximum is sharp, and intensity is high, almost has no other impurity peaks appearance, illustrates its purity is high, crystallization
Property is good.
Embodiment 2
Step 1: the oxalic acid for weighing 5mmol dissolves in the going in ethylene glycol of 40mL, and two drop ammonium hydroxide are added dropwise, after magnetic agitation 30min
To solution A；Weigh the V of 2mmol2O5It is dissolved in solution A, magnetic agitation 30min obtains solution B.
Step 2: configured solution B is poured into reaction polytetrafluoroethyllining lining, and the packing ratio of reaction kettle is 80%, and
Liner is fitted into outer kettle, is placed it in baking oven after fixing, reaction condition is to keep the temperature for 24 hours at 200 DEG C.
Step 3: water heating kettle cooled to room temperature after to hydro-thermal reaction pours out reaction solution deionized water, anhydrous
Ethyl alcohol is respectively washed 3 times.By sample collection and dry 12h under the conditions of 80 DEG C of vacuum after suction filtration, VO2 nano material can be obtained.
Step 4: the molar ratio of control barium oxide and sublimed sulfur is 1:9, and two kinds of raw materials are laid in porcelain boat two respectively
End, porcelain boat is placed in tube-type atmosphere furnace, and in two furnace plugs of pipe both ends each side.
Step 5: being passed through inert gas into pipe, then carries out 5 pumping tonifying Qi, drains inner air tube, and last time is taken out
No longer tonifying Qi after gas, control intraductal atmospheric pressure are -1 ~ 0MPa；When air pressure is -1 ~ 0MPa, with the heating speed of 5 ~ 10 DEG C/min
Rate rises to 800 DEG C, and keeps the temperature 2h；After heat preservation, air valve is opened immediately, inert gas is passed through with 700 ~ 800sccm air-flow, is arranged
The sulfur vapor generated in insulating process out will guarantee that cooling carries out under argon gas stream later.
Step 6: calcined samples with water and dehydrated alcohol are respectively washed 3 times, and drying for 24 hours, can be obtained at 60 DEG C
V3S4 nano material.
Fig. 3 is VO prepared by the embodiment of the present invention 22Scanning electron microscope (SEM) map；It can be seen that prepared by example 2
VO2Pattern be thin rodlike.
Embodiment 3
Step 1: the oxalic acid for weighing 5mmol dissolves in the deionized water of 40mL, and four drop ammonium hydroxide are added dropwise, after magnetic agitation 30min
To solution A；Weigh the V of 2mmol2O5It is dissolved in solution A, magnetic agitation 30min obtains solution B.
Step 2: configured solution B is poured into reaction polytetrafluoroethyllining lining, and the packing ratio of reaction kettle is 80%, and
Liner is fitted into outer kettle, is placed it in baking oven after fixing, reaction condition is to keep the temperature for 24 hours at 180 DEG C.
Step 3: water heating kettle cooled to room temperature after to hydro-thermal reaction pours out reaction solution deionized water, anhydrous
Ethyl alcohol is respectively washed 3 times.It is dried for 24 hours by sample collection after suction filtration and under the conditions of 40 DEG C of vacuum, VO can be obtained2Nano material.
Step 4: the molar ratio of control barium oxide and thioacetamide is 1:12, and two kinds of raw materials are laid in porcelain respectively
Boat both ends, porcelain boat is placed in tube-type atmosphere furnace, and in two furnace plugs of pipe both ends each side.
Step 5: being passed through inert gas into pipe, then carries out 8 pumping tonifying Qi, drains inner air tube, and last time is taken out
No longer tonifying Qi after gas, control intraductal atmospheric pressure are -1 ~ 0MPa；When air pressure is -1 ~ 0MPa, with the heating rate of 5 DEG C/min
700 DEG C are risen to, and keeps the temperature 3h；After heat preservation, air valve is opened immediately, inert gas is passed through with 700 ~ 800sccm air-flow, is discharged
The sulfur vapor generated in insulating process will guarantee that cooling carries out under argon gas stream later.
Step 6: calcined samples with water and dehydrated alcohol are respectively washed 3 times, and dry 12h, can be obtained at 80 DEG C
V3S4Nano material.
Fig. 4 is V prepared by the embodiment of the present invention 33S4Scanning electron microscope (SEM) map；It can be seen that prepared by example 3
V3S4Pattern be laminar.
Embodiment 4
Step 1: the oxalic acid for weighing 4mmol dissolves in the deionized water and ethylene glycol (1:1) of 40mL, and two drop ammonium hydroxide, magnetic force is added dropwise
Solution A is obtained after stirring 30min；Weigh the V of 2mmol2O5It is dissolved in solution A, magnetic agitation 30min obtains solution B.
Step 2: configured solution B is poured into reaction polytetrafluoroethyllining lining, and the packing ratio of reaction kettle is 80%, and
Liner is fitted into outer kettle, is placed it in baking oven after fixing, reaction condition is to keep the temperature 20h at 200 DEG C.
Step 3: water heating kettle cooled to room temperature after to hydro-thermal reaction pours out reaction solution deionized water, anhydrous
Ethyl alcohol is respectively washed 3 times.It is dried for 24 hours by sample collection after suction filtration and under the conditions of 60 DEG C of vacuum, VO can be obtained2Nano material.
Step 4: the molar ratio of control barium oxide and thiocarbamide is 1:11, and two kinds of raw materials are laid in porcelain boat both ends respectively,
Porcelain boat is placed in tube-type atmosphere furnace, and in two furnace plugs of pipe both ends each side.
Step 5: being passed through inert gas into pipe, then carries out 8 pumping tonifying Qi, drains inner air tube, and last time is taken out
No longer tonifying Qi after gas, control intraductal atmospheric pressure are -1 ~ 0MPa；When air pressure is -1 ~ 0MPa, with the heating rate of 10 DEG C/min
900 DEG C are risen to, and keeps the temperature 2h；After heat preservation, air valve is opened immediately, inert gas is passed through with 800 ~ 900sccm air-flow, is discharged
The sulfur vapor generated in insulating process will guarantee that cooling carries out under argon gas stream later.
Step 6: calcined samples with water and dehydrated alcohol are respectively washed 3 times, and dry 12h, can be obtained at 80 DEG C
V3S4Nano material.
Fig. 5 is V prepared by the embodiment of the present invention 43S4Production hydrogen test chart (LSV) map in an acidic solution；It can be seen that
V prepared by example 43S4, under the test condition of pH=0, when current density is 10mA/cm2, should when sweep speed is 5 mV/s
Sample overpotential is 375mV, there is certain production hydrogen catalysis activity.
Fig. 6 is V prepared by the embodiment of the present invention 43S4Production hydrogen test chart (LSV) map in neutral solution；It can be seen that
V prepared by example 43S4, under the test condition of pH=7, when current density is 10mA/cm2, should when sweep speed is 5 mV/s
Sample overpotential is 390mV, there is certain production hydrogen catalysis activity.
Fig. 7 is V prepared by the embodiment of the present invention 43S4Production hydrogen test chart (LSV) map in alkaline solution；It can be seen that
V prepared by example 43S4, under the test condition of pH=14, when current density is 10mA/cm2, should when sweep speed is 5 mV/s
Sample overpotential is 465mV, there is certain production hydrogen catalysis activity.
Claims (10)
1. a kind of sheet V3S4The preparation method of elctro-catalyst, which comprises the following steps:
Hydro-thermal reaction will be carried out containing the alkaline solution in vanadium source, oxalic acid, obtains a kind of barium oxide nano material；By a kind of vanadium oxygen
Compound nano material and sulphur source are according to molar ratio 1:(9 ~ 12) 700-900 DEG C of calcining under an inert atmosphere, obtain sheet V3S4Electricity is urged
Agent.
2. a kind of sheet V according to claim 13S4The preparation method of elctro-catalyst, which is characterized in that the vanadium source is
V2O5；The sulphur source is the one or more of sublimed sulfur, thioacetamide, thiocarbamide.
3. a kind of sheet V according to claim 13S4The preparation method of elctro-catalyst, which is characterized in that will containing vanadium source,
The alkaline solution of oxalic acid is obtained by method comprising the following steps: being first uniformly mixed organic acid with solvent, is prepared concentration of oxalic acid
For the solution of 0.01 ~ 0.15mol/L；The pH value for adjusting oxalic acid is alkalinity；Vanadium source substance is added, it is equal to mixing to continue stirring
It is even.
4. a kind of sheet V according to claim 33S4The preparation method of elctro-catalyst, which is characterized in that described to contain
Vanadium source, oxalic acid alkaline solution pH value be 7.8 ~ 10.3；The process for adjusting pH value is to be added dropwise, and is stirred after a drop ammonium hydroxide is added
It mixes to solution PH and does not change, a drop of then dripping, until the last pH value of solution reaches target value.
5. a kind of sheet V according to claim 33S4The preparation method of elctro-catalyst, which is characterized in that the solvent is
One of deionized water, ethyl alcohol, ethylene glycol, isopropanol are a variety of.
6. a kind of sheet V according to claim 13S4The preparation method of elctro-catalyst, which is characterized in that hydro-thermal reaction
Packing ratio is 80%, reaction temperature be 180 DEG C ~ 200 DEG C, the reaction time be 20 ~ for 24 hours.
7. a kind of sheet V according to claim 13S4The preparation method of elctro-catalyst, which is characterized in that before calcining, to anti-
It answers container to be passed through inert gas, then carries out 3 ~ 10 pumping tonifying Qi, drain container atmosphere, last time is no longer mended after being evacuated
Gas, control intraductal atmospheric pressure are -1 ~ 0MPa.
8. a kind of sheet V according to claim 13S4The preparation method of elctro-catalyst, which is characterized in that calcination condition are as follows:
When air pressure is -1 ~ 0MPa, 700 ~ 900 DEG C are risen to the heating rate of 5 ~ 10 DEG C/min, and keep the temperature 2 ~ 3h；Heat preservation terminates
Afterwards, air valve is opened immediately, and inert gas is passed through with 500 ~ 1500sccm air-flow, the sulfur vapor generated in insulating process is discharged, it
After to guarantee cooling carried out under inert atmosphere stream.
9. a kind of sheet V of any one of claim 1 ~ 8 the method preparation3S4Elctro-catalyst.
10. a kind of sheet V described in claim 93S4Elctro-catalyst answering in terms of cracking aquatic products hydrogen catalyst as electro-catalysis
With.
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| CN201811591304.4A CN109706479B (en) | 2018-12-25 | 2018-12-25 | Sheet V3S4Preparation of (A) and application of electrocatalytic properties thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110137460A (en) * | 2019-05-09 | 2019-08-16 | 济南大学 | A kind of hollow V of lithium/sodium ions to potassium ions battery3S4The preparation method of@C nano pipe negative electrode material |
| CN111203254A (en) * | 2020-01-13 | 2020-05-29 | 陕西科技大学 | Co-N high-activity species modified vanadium sulfide hydrogen-producing electrocatalyst and preparation method and application thereof |
| CN113413906A (en) * | 2021-07-30 | 2021-09-21 | 陕西科技大学 | Vanadium trisulfide/graphite phase carbon nitride photocatalyst and preparation method thereof |
| CN116377504A (en) * | 2023-06-01 | 2023-07-04 | 中石油深圳新能源研究院有限公司 | Hydrogen and oxygen evolution catalyst, preparation method thereof, electrolysis device and electrode thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110137460A (en) * | 2019-05-09 | 2019-08-16 | 济南大学 | A kind of hollow V of lithium/sodium ions to potassium ions battery3S4The preparation method of@C nano pipe negative electrode material |
| CN110137460B (en) * | 2019-05-09 | 2022-02-01 | 济南大学 | Hollow V for lithium/sodium/potassium ion battery3S4Preparation method of @ C nanotube negative electrode material |
| CN111203254A (en) * | 2020-01-13 | 2020-05-29 | 陕西科技大学 | Co-N high-activity species modified vanadium sulfide hydrogen-producing electrocatalyst and preparation method and application thereof |
| CN111203254B (en) * | 2020-01-13 | 2023-01-31 | 陕西科技大学 | Co-N high-activity species modified vanadium sulfide hydrogen-producing electrocatalyst and preparation method and application thereof |
| CN113413906A (en) * | 2021-07-30 | 2021-09-21 | 陕西科技大学 | Vanadium trisulfide/graphite phase carbon nitride photocatalyst and preparation method thereof |
| CN116377504A (en) * | 2023-06-01 | 2023-07-04 | 中石油深圳新能源研究院有限公司 | Hydrogen and oxygen evolution catalyst, preparation method thereof, electrolysis device and electrode thereof |
| CN116377504B (en) * | 2023-06-01 | 2023-09-01 | 中石油深圳新能源研究院有限公司 | Hydrogen and oxygen evolution catalyst, preparation method thereof, electrolysis device and electrode thereof |
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